一种​香草醛​分子​印迹​材料​的​制备​方​法及​应用

源语言标题
(CN105968401) 一种​香草醛​分子​印迹​材料​的​制备​方​法及​应用
公开号/公开日
CN105968401 A 2016-09-28 [CN105968401] / 2016-09-28
申请号/申请日
2016CN-0323371 / 2016-05-10
发明人
SU LIQIANG;ZOU XUEYING;BAI JINFENG;LI JING;ZU GUANGQUAN;
申请人
QIQIHAR UNIVERSITY;
主分类号
IPC分类号
B01J-020/26B01J-020/30C08F-292/00C08J-009/26C08L-051/10
摘要
(CN105968401) 本​发明​涉及​种​香草醛​的​分子​印迹​材料​的​制备​方​法及​应用,具体​步骤​如下:通过​紫外​可见​分光​光度​法​对​模板​分子​与​功能​单体​的​比例​进行​选择;将​定量​的​埃洛​石​加​至​盐酸​溶液​中​进行​活化,在​无水​甲苯​中​充​氮​排​氧​加热​密封​的​条件下,加入​硅​烷​偶​联​剂​γ‑甲基​丙烯​酰​氧​基​丙基​三甲​氧​基​硅​烷(KH‑570)进行​反应,完成​改性;将上​述​改性​埃洛​石​分散​于​乙​腈​溶剂​中,加入​预​聚合​的​香草醛​和​功能​单体,再加入​分散剂、交​联​剂​及​引发​剂​加热​条件下​进行​聚合反应,经​索​氏​提取​除去​模板,从而​制备​出​所需​的​基于​埃洛​石​的​香草醛​分子​印迹​材料,该​材料​对​香草醛​具有​较强​的​特异​识别​能力、较高​的​吸附​量等​优点,可以​实现​分离​并​富集​食品​样品​中​香草醛​的​目的,具有​定的​实际应用​价值。
地址
代理人
代理机构
;
优先权号
2016CN-0323371 2016-05-10
主权利要求
(CN105968401) 1. Method of preparing one vanillylaldehyde molecularly imprinted material, characterized in, which comprises the steps of: The selection of the template molecule (1) and the functional monomer ratio A template molecule vanillylaldehyde and functional monomers -methyl acrylic acid molar ratio of 1: 0.001-1: 8; Preparation of activated (2) halioysite Using a sieve particle size of 180 1g: 10 ml volume ratio by mass is added to halioysite object 2-6 mol/L hydrochloric acid solution was activated 12-24h, suction filtration and washed with distilled water until neutral, dried in a vacuum oven for backup; Hvdrosilylation (3) halioysite m-HNTs preparation In the 120mL60-70 Ć anhydrous toluene solution, prepared (2) by adding 0.5-2 g of activated halioysite, 10-30 ml silane coupling agent KH-570, a nitrogen-filled hermetically sealed; agitating the reaction 24-36h, after completion of the reaction, respectively with toluene, acetone, ethyl Nitrile suction washed, and incubated at 50-60 Ć vacuum drying, resulting silanized halioysite m-HNTs; Imprinted material (4) of prepolymerization The template molecule vanillylaldehyde to the functional monomer -methyl acrylic acid molar ratio of 1:4 in acetonitrile prepolymerization 12-24h, a self-assembled with a monomer solution to obtain a template; Molecularly imprinted material preparation of vanillylaldehyde (5) The step (3) of the resulting m-HNTs dispersed in acetonitrile solution, in accordance with vanillylaldehyde: -methyl acrylic acid: ethylene glycol dimethacrylate esters moore 1:4 ratio: (16-20), at a concentration of 10-12.5 mmol/L per milliliter of solution vanillylaldehyde, polyvinylpyrrolidone 0.2-0.4 g sequentially adding a dispersing agent, a crosslinking agent ethylene glycol dimethacrylate and an initiator such as azobisisobutyronitrile 0.03-0.08 g even agent, at 60-70 Ć under conditions of reaction was stirred for 18-24h; is then the product was washed with ethyl Nitrile suction, and is dried to constant weight in a vacuum oven; Removal of template molecule (6) Methanol/acetic acid mixture of the polymer was subjected to Soxhlet extraction, a temperature control 80-100 Ć, extracting 18-36h, to remove the template molecule, the product was dried over anhydrous methanol, distilled water washed to pH=7 crosses, vacuum drying to constant weight, molecularly imprinted materials vanillylaldehyde surface halioysite obtained.  3. Method of producing a non-imprinted materials, characterized in, which comprises the steps of: Preparation of activated (1) halioysite Using a sieve particle size of 180 1g: 10 ml volume ratio by mass is added to halioysite object 2-6 mol/L hydrochloric acid solution was activated 12-24h, suction filtration and washed with distilled water until neutral, dried in a vacuum oven for backup; Hvdrosilylation (2) halioysite m-HNTs preparation In a 120 ml 60-70 Ć anhydrous toluene solution, prepared (2) by adding 0.5-2 g of activated halioysite, 10-30 ml silane coupling agent KH-570, a nitrogen-filled hermetically sealed; agitating the reaction 24-36h, after completion of the reaction, respectively with toluene, acetone, ethyl Nitrile suction washed, and incubated at 50-60 Ć vacuum drying, resulting silanized halioysite m-HNTs; Preparation of a non- (3) imprinted material The step (2) of the resulting m-HNTs dispersed in acetonitrile solution, in accordance with -methyl acrylic acid: ethylene glycol dimethacrylate esters moore ratio 4: (16-20), sequentially add the dispersant polyvinylpyrrolidone 0.2-0.4 g, a crosslinking agent ethylene glycol dimethacrylate and an initiator such as azobisisobutyronitrile 0.03-0.08 g even agent, at 60-70 Ć under conditions of reaction was stirred for 18-24h; is then the product was washed with ethyl Nitrile suction, and is dried to constant weight in a vacuum oven; obtaining a non-imprinted material.  4. Molecularly imprinted material vanillylaldehyde A method of application, characterized in, which comprises the steps of: 3 ml of filter plates were weighed in a 50 mg MIP loaded with polypropylene void volume, made molecularly imprinted solid phase extraction pillar (MISPE); solid-phase extraction experiments on two actual sample, ultrahigh performance liquid chromatography loading solution and a concentrated solution (UPLC) detection.
法律状态
(CN105968401) LEGAL DETAILS FOR CN105968401  Actual or expected expiration date=2036-05-10    Legal state=ALIVE    Status=PENDING     Event publication date=2016-05-10  Event code=CN/APP  Event indicator=Pos  Event type=Examination events  Application details  Application country=CN CN201610323371  Application date=2016-05-10  Standardized application number=2016CN-0323371     Event publication date=2016-09-28  Event code=CN/A  Event type=Examination events  Published application  Publication country=CN  Publication number=CN105968401  Publication stage Code=A  Publication date=2016-09-28  Standardized publication number=CN105968401     Event publication date=2016-09-28  Event code=CN/C06  Event indicator=Pos  Event type=Examination events  Publication    Event publication date=2016-10-26  Event code=CN/C10  Event type=Examination events  Request of examination as to substance
专利类型码
A
国别省市代码
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